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Simultaneous quantitation of folic acid and 5-methyltetrahydrofolic acid in human plasma by HPLC-MS/MS and its application to a pharmacokinetic study☆

Xiaohong ZHENG ; Liyuan JIANG ; Lanting ZHAO ; Quanying ZHANG ; Li DING

Journal of Pharmaceutical Analysis.2015;5(4):269-275. doi:10.1016/j.jpha.2015.05.004

A sensitive method based on high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the simultaneous determination of folic acid (FA) and its active metabolite, 5-methyltetrahydrofolic acid (5-M-THF), in human plasma. The analytes were extracted from plasma with methanol solution containing 10 mg/mL of 2-mercaptoethanol and 0.025% (v/v) ammonium hydroxide. FA and 5-M-THF were more stable after the addition of 2-mercaptoethanol and ammonium hydroxide in the sample preparation procedures of this study than they were in the previously published methods. Chromatographic separation was performed on a Hedera ODS-2 column using a gradient elution system of acetonitrile and 1 mM ammonium acetate buffer solution containing 0.6% formic acid as mobile phase. LC-MS/MS was carried out with an ESI ion-source and operated in the multiple reaction monitoring (MRM) mode. The assay was linear over the concentration ranges of 0.249-19.9 ng/mL for FA, and 5.05-50.5 ng/mL for 5-M-THF. The developed LC-MS/MS method offers increased sensitivity for quantification of FA and 5-M-THF in human plasma and was applicable to a pharmacokinetic study of FA and 5-M-THF.

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Simultaneous determination of four Sudan dyes in rat blood by UFLC-MS/MS and its application to a pharmacokinetic study in rats☆

Hao ZHU ; Yijun CHEN ; Changshun HUANGA ; Yangyang HAN ; Yiwei ZHANG ; Shucan XIE

Journal of Pharmaceutical Analysis.2015;5(4):239-248. doi:10.1016/j.jpha.2015.03.001

A rapid and sensitive method based on ultrafast liquid chromatography-tandem mass spectrometry was developed and validated for simultaneous determination of Sudan Ⅰ, Sudan Ⅱ, Sudan Ⅲ, and Sudan Ⅳ levels in rat whole blood. Cleanert C18 mixed-mode polymeric sorbent was used for effective solid-phase extraction cleanup. Separation was carried out on a reversed-phase C18 column (100 mm × 2.1 mm, 1.8 μm) using 0.1% (v/v) formic acid in water/0.1% (v/v) formic acid in acetonitrile as the mobile phase in gradient elution. Quantification was performed by an electrospray ionization source in the positive multiple reaction monitoring mode using D5-Sudan I as the internal standard. Calibration curves showed good linearity between 0.2 and 20.0 μg/L, with correlation coefficients higher than 0.9990. The average recovery rates were between 93.05% and 114.98%. The intra- and inter-day relative standard deviations were within 6.2%. The lower limit of quantification was 0.2 μg/L. All the analytes were found to be stable in aseries of stability studies. The proposed method was successfully applied to a pharmacokinetic study of four Sudan dyes after oral administration to rats.

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Development and validation of a GC-FID method for quantitative analysis of oleic acid and related fatty acids☆

Honggen ZHANG ; Zhenyu WANG ; Oscar LIU

Journal of Pharmaceutical Analysis.2015;5(4):223-230. doi:10.1016/j.jpha.2015.01.005

Oleic acid is a common pharmaceutical excipient that has been widely used in various dosage forms. Gas chromatography (GC) has often been used as the quantitation method for fatty acids normally requiring a derivatization step. The aim of this study was to develop a simple, robust, and derivatization-free GC method that is suitable for routine analysis of all the major components in oleic acid USP-NF (United States Pharmacopeia-National Formulary) material. A gas chromatography-flame ionization detection (GC-FID) method was developed for direct quantitative analysis of oleic acid and related fatty acids in oleic acid USP-NF material. Fifteen fatty acids were separated using a DB-FFAP (nitroterephthalic acid modified polyethylene glycol) capillary GC column (30 m × 0.32 mm i.d.) with a total run time of 20 min. The method was validated in terms of specificity, linearity, precision, accuracy, sensitivity, and robustness. The method can be routinely used for the purpose of oleic acid USP-NF material analysis.

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Determination of atractylon in rat plasma by a GC-MS method and its application to a pharmacokinetic study

Han YAN ; Yuanyuan SUN ; Yuying MA ; Bin JI ; Xiaohong HOU ; Zhiguo YU ; Yunli ZHAO

Journal of Pharmaceutical Analysis.2015;5(5):327-331. doi:10.1016/j.jpha.2015.03.002

A sensitive and selective method based on gas chromatography hyphenated to mass spectrometry (GC-MS) was developed and validated for the determination of atractylon in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate-n-hexane (1:1, v/v) using acetophenone as an internal standard (IS). Analytes were determined in selective ion monitoring (SIM) mode using target ions at m/z 108.1 for atractylon and m/z 105.1 for acetophenone. The calibration curve was linear over the concentration range of 10-1000 ng/mL with lower limit of quantification of 10 ng/mL. The intra- and inter-day precision variations were not more than 10.4% and 9.6%, respectively, whilst accuracy values ranged from -6.5% to 4.9%. Extraction recovery of the assay was satisfactory. This method was suc-cessfully applied to quantification and pharmacokinetic study of atractylon in rat plasma after in-tragastric administration of Atractylodis extract.

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High-sensitivity simultaneous liquid chromatography-tandem mass spectrometry assay of ethinyl estradiol and levonorgestrel in human plasma

Abhishek GANDHI ; Swati GUTTIKAR ; Priti TRIVEDI

Journal of Pharmaceutical Analysis.2015;5(5):316-326. doi:10.1016/j.jpha.2015.02.002

A sensitive and simultaneous liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of ethinyl estradiol and levonorgestrel. The analytes were extracted with methyl-tert-butyl ether: n-hexane (50:50, v/v) solvent mixture, followed by dansyl derivatization. The chromatographic separation was performed on a Kinetex C18 (50 mm × 4.6 mm, 2.6μm) column with a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile in gradient composition. The mass transitions were monitored in electrospray positive ionization mode. The assay exhibited a linear range of 0.100-20.0 ng/mL for levonorgestrel and 4.00-500 pg/mL for ethinyl estradiol in human plasma. A run time of 9.0 min for each sample made it possible to analyze a throughput of more than 100 samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic and bioequivalence studies.

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Four new degradation products of doxorubicin:An application of forced degradation study and hyphenated chromatographic techniques

Dheeraj KAUSHIK ; Gulshan BANSAL

Journal of Pharmaceutical Analysis.2015;5(5):285-295. doi:10.1016/j.jpha.2015.05.003

Forced degradation study on doxorubicin (DOX) was carried out under hydrolytic condition in acidic, alkaline and neutral media at varied temperatures, as well as under peroxide, thermal and photolytic conditions in accordance with International Conference on Harmonization (ICH) guidelines Q1(R2). It was found extremely unstable to alkaline hydrolysis even at room temperature, unstable to acid hy-drolysis at 80 °C, and to oxidation at room temperature. It degraded to four products (O-I-O-IV) in oxidative condition, and to single product (A-I) in acid hydrolytic condition. These products were re-solved on a C8 (150 mm × 4.6 mm, 5μm) column with isocratic elution using mobile phase consisting of HCOONH4 (10 mM, pH 2.5), acetonitrile and methanol (65:15:20, / / ). Liquid chromatography-pho-todiode array (LC-PDA) technique was used to ascertain the purity of the products noted in LC-UV chromatogram. For their characterization, a six stage mass fragmentation (MS6) pattern of DOX was outlined through mass spectral studies in positive mode of electrospray ionization (+ESI) as well as through accurate mass spectral data of DOX and the products generated through liquid chromato-graphy-time of flight mass spectrometry (LC-MS-TOF) on degraded drug solutions. Based on it, O-I-O-IV were characterized as 3-hydroxy-9-desacetyldoxorubicin-9-hydroperoxide, 1-hydroxy-9-desacetyldox-orubicin-9-hydroperoxide, 9-desacetyldoxorubicin-9-hydroperoxide and 9-desacetyldoxorubicin, re-spectively, whereas A-I was characterized as deglucosaminyl doxorubicin. While A-I was found to be a pharmacopoeial impurity, all oxidative products were found to be new degradation impurities. The mechanisms and pathways of degradation of doxorubicin were outlined and discussed.

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Species authentication and geographical origin discrimination of herbal medicines by near infrared spectroscopy:A review

Zhiguo YU

Journal of Pharmaceutical Analysis.2015;5(5):277-284. doi:10.1016/j.jpha.2015.04.001

Near infrared (NIR) spectroscopy as a rapid and nondestructive analytical technique, integrated with chemometrics, is a powerful process analytical tool for the pharmaceutical industry and is becoming an attractive complementary technique for herbal medicine analysis. This review mainly focuses on the recent applications of NIR spectroscopy in species authentication of herbal medicines and their geo-graphical origin discrimination.

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Development of an HPLC-UV assay method for the simultaneous quantification of nine antiretroviral agents in the plasma of HIV-infected patients

Nitin CHARBE ; Sara BALDELLI ; Valeria COZZI ; Simone CASTOLDI ; Dario CATTANEO ; Emilio CLEMENTI

Journal of Pharmaceutical Analysis.2016;6(6):396-403.

A new method using high-performance liquid chromatography coupled with ultra violet detection (HPLC–UV) was developed and validated for the simultaneous quantification of atazanavir, dolutegravir, darunavir, efavirenz, etravirine lopinavir, raltegravir, rilpivirine and tipranavir in human plasma. For the first time we reported here the development and validation of an HPLC–UV assay to quantify the frequently administered 9 antiretroviral compounds including dolutegravir and rilpivirine. A simple solid phase extraction procedure was applied to 500 μL aliquots of plasma. The chromatographic separation of the drugs and internal standard (quinoxaline) was achieved with a gradient of acetonitrile and sodium acetate buffer on a C18 reverse-phase analytical column with a 25 min analytical run time. Calibration curves were optimised according to the therapeutic range of drug concentrations in patients, and the coefficient of determination (r2) was higher than 0.99 for all analytes. Mean intraday and interday precisions (RSD) for all compounds were less than 15.0%, and the mean accuracy (%deviation from nominal concentration) was also found to be less than 15.0%. Extraction recovery range was between 80%and 120%for all drugs analysed. The solid phase extraction and HPLC–UV method enable a specific, sensitive, and reliable simultaneous determination of nine antiretroviral agents in plasma. Good extraction efficiency and low limit of HPLC–UV quantification make this method suitable for use in clinical trials and therapeutic drug monitoring.

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Optimization of microwave-assisted extraction of bioactive alkaloids from lotus plumule using response surface methodology☆

Wei XIONG ; Xianqiang CHEN ; Guangping LV ; Dejun HU ; Jing ZHAO ; Shaoping LI

Journal of Pharmaceutical Analysis.2016;6(6):382-388.

In this work, a fast and efficient microwave-assisted extraction (MAE) method was developed to extract main bioactive alkaloids from lotus plumue. To optimize MAE conditions, three main factors were selected using univariate approach experiments, and then central composite design (CCD). The optimal extraction conditions were as follows: methanol concentration of 65%, microwave power of 200 W, and extraction time of 260 s. A high performance liquid chromatography–diode array detector (HPLC–DAD) method was established to quantitatively analyze these phytochemicals in different lotus plumule samples and in different part of lotus. Chromatographic separation was carried out on an Agilent Zorbax Extend-C18 column (4.6 mm×150 mm, 3.5 μm). Gradient elution was applied with the mobile phase constituted with 0.1%triethylamine in water (A) and acetonitrile (B): 40%?70% B at 0?8 min, 70%?100% B at 8–9 min, 100% B for 2 min, and then equilibrated with 40%B for 2 min.

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Comparison of ESI-and APCI-LC-MS/MS methods:A case study of levonorgestrel in human plasma☆

Rulin WANG ; Lin ZHANG ; Zunjian ZHANG ; Yuan TIAN

Journal of Pharmaceutical Analysis.2016;6(6):356-362.

Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) techniques for liquid chromatography–tandem mass spectrometry (LC–MS/MS) determination of levonorgestrel were evaluated. In consideration of difference in ionization mechanism, the two ionization sources were compared in terms of LC conditions, MS parameters and performance of method. The sensitivity for detection of levonorgestrel with ESI was 0.25 ng/mL which was lower than 1 ng/mL with APCI. Matrix effects were evaluated for levonorgestrel and canrenone (internal standard, IS) in human plasma, and the results showed that APCI source appeared to be slightly less liable to matrix effect than ESI source. With an overall consideration, ESI was chosen as a better ionization technique for rapid and sensitive quantification of levonorgestrel. The optimized LC–ESI–MS/MS method was validated for a linear range of 0.25–50 ng/mL with a correlation coefficient≥0.99. The intra-and inter-batch precision and accuracy were within 11.72%and 6.58%, respectively. The application of this method was demonstrated by a bioequivalence study following a single oral administration of 1.5 mg levonorgestrel tablets in 21 Chinese healthy female volunteers.

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